Tube uniting with fusion barrier

ABSTRACT

The invention herein described was made in the course of or under a contract or subcontract thereunder with the Department of the Army. An illustrative embodiment of the invention is directed to method and apparatus for manufacturing microchannel devices. Typically, individual glass tubes are suspended vertically in a furnace. A vacuum is drawn within the furnace so that the inner surfaces of the tubes, exposed to atmospheric pressure, will not collapse during heating and drawing. At temperature, the bundle is drawn in order to elongate and reduce the bundle cross section by a ratio of about 50 to 1. The elongated bundle is cut into lengths that are stacked together within a tube of glass that has a higher melting point than the glass in the drawn lengths. The channels are once more sealed and the adjacent hexagonal lengths are subjected to a secondary fusion process prior to slicing into thin discs. To prevent the inner lengths from cracking during cooling, the inner surface of the tube is treated with a fusion inhibiting compound (e.g., boron nitride).

United States Patent [72] Inventor Horst G. Fleck San Antonio, Tex.

[21 Appl. No. 830,008

[22] Filed June 3, 1969 [45] Patented Nov. 23, 1971 [73] Assignee Weston Instruments, Inc.

Newark, NJ.

[54] TUBE UNITING WITH FUSION BARRIER 1 Claim, 7 Drawing Figs.

[521 US. Cl 65/4, 65/12, 65/24,65/26,65/110, 65/156 [5 l Int. Cl ..C03c 23/20, C03b 39/00 [50] Field of Search 65/D1G. 7, 4, 12, 89, 86, 24,26,110, 156

[56] References Cited UNITED STATES PATENTS 3,269.817 8/1966 Bondley 65/4 X 3,275,428 9/1966 Siegmund 65/4 3.331.670 7/1967 Cole 65/4 3,455,666 7/1969 Bazinet', .Ir... 65/4 1,169,681 1/1916 Sand 65/D1G. 7 1,410,741 3/1922 Erdle 65/4 X 1,793,529 2/1931 Taylor... 65/4 X 2,313,296 3/1943 Lamesh 65186 X 2,433,116 12/1947 Greenbowc et 111.... 65/89X 3,182,394 5/1965 Jentzsch 65/D1G. 7

POWER SUPPLY Primary Examiner-Frank W. Miga Attorneys-William R. Sherman, Donald H. Fidler, Stewart F.

Moore and John P. Sinnott ABSTRACT: The invention herein described was made in the course of or under a contract or subcontract thereunder with the Department of the Army. An illustrative embodiment of the invention is directed to method and apparatus for manufacturing microchannel devices. Typically, individual glass tubes are suspended vertically in a furnace. A vacuum is drawn within the furnace so that the inner surfaces of the tubes, exposed to atmospheric pressure, will not collapse during heating and drawing. At temperature, the bundle is drawn in order to elongate and reduce the bundle cross section by a ratio of about 50 to 1. The elongated bundle is cut into lengths that are stacked together within a tube of glass that has a higher melting point than the glass in the drawn lengths.

The channels are once more sealed and the adjacent hexagonal lengths are subjected to a secondary fusion process prior to slicing into thin discs. To prevent the inner lengths from cracking during cooling, the inner surface of the tube is treated with a fusion inhibiting compound (e.g., boron nitride).

*TO VACUUM PUMP GRADI ENT CONTROL PATENTEDunv 23 IBTI 3,622 292 sum 1 0r 4 TO VACUUM PUMP FURNACE EMPERATUR GRADIENT CONTROL POWER SUPPLY INVENTOR.

Horsr G. Fleck ,A'I'TORNEY PATENTEDNUV 23 I97] SHEET 2 BF 4 PATENTEU 23 197i 3, 622,292

SHEET 3 OF 4 PHOTOMULTIPLIER TUBE 5 TO MOTORS 22 AND 33 (F|G.1)

MOTOR SPEED CONTROL CIRCUIT A rum; UNITING wrrrr FUSION BARRIER BACKGROUND OF THE INVENTION 1. Field of the Invention This invention relates to manufacturing techniques, and more particularly, to method and apparatus for producing microchannel devices, and the like.

2. Description of the Prior Art A need exists for microstructure discs in which the microchannels are arranged generally perpendicular to the disc sides. Microchannel devices are useful, for example, in channel electron multipliers and in chemical filters. Ideally, a channel electron multiplier for use in an image intensifier might contain thousands of pores in a disc that is about I/ of an inch thick. The individual channels, moreover, ought to be each on the order of hundredths of an inch in diameter to provide a length to diameter ratio of approximately 50 to I.

In order to manufacture structures of this sort, it has been suggested to arrange a bundle of glass rods in which each rod has an outer annulus and an inner core of different glasses. The bundle is heated and allowed to elongate under gravitational force until the desired individual channel diameters are achieved. On cooling, transverse slices in the drawn structure produce discs of the proper thickness. The solid inner core in each rod is dissolved in an acid that attacks the core glass without affecting the annular glass. This technique has been unsatisfactory, however, because the acid does not produce an array of cylindrical microchannels but instead generates undesirable passageways that have generally hyperbolic cross sections.

This solid core technique has been proposed in order to overcome the natural tendency of hollow glass tubes to collapse during the hot drawing process. Especially during a final or secondary fusion step, the tubes that form the mutually abutting boundaries of individual hexagonal elements often collapse and produce a chicken wire appearance on the surface of the disc. This, of course, is an intolerable defect for most applications and leads to a production run that must be discarded.

Accordingly, a need exists for a microchannel production technique that enables hollow tubes to be used throughout, without allowing these tubes to collapse during processing.

SUMMARY OF THE INVENTION These problems are overcome through a differential pressure technique in which the air pressure within the channels is greater than the pressure in the furnace in order to prevent tube collapse during a two-stage heating and drawing process. During the primary draw, an end of each of the glass tubes is sealed. The tubes are suspended in a vacuum furnace from hangers that are fused in the sealed ends. After mounting, the tube support structure is evacuated.

The furnace has a temperature gradient that produces the greatest heat at the top to prevent air circulation during drawing. At the proper temperature, the glass bundle starts to flow under the control of a modified Atwoods machine, in which the weight of the bundle is counterbalanced by means of an equivalent weight at the other end of a system of sheaves in order to eliminate the influence of gravity. As the tube bundle flow progresses, the length of the bundle within the support structure is changed. The temperature gradient also may be adjusted in a corresponding manner to insure that the portion of the bundle remaining in the furnace is subjected to the proper temperature. Preferably, however, the established temperature condition in the furnace is maintained constant and the rate of flow is adjusted through the control of a drawing mechanism. Typically, the feed rate of the bundle into the furnace is regulated visually to keep fixed the vertical position of the bundles transitional portion (that zone in which diameter reduction and bundle elongation commences).

The drawn portion of each bundle is cut into individual lengths. These lengths are grouped into another bundle to produce an array of several tens of thousands of hollow tubes.

Both ends of the tubes in each of the primary lengths in this array are sealed in order to entrap air at atmospheric pressure in the microchannels.

The array is then placed inside a larger glass tube that has a somewhat higher melting point and slightly lower coefficient of thermal expansion than the glass from which the microchannels are made. To prevent void spaces from forming between the polygonlike periphery of the array of primary lengths and the cylindrical inner surface of the circumscribing glass tube, solid filling rods are inserted in the gaps.

In accordance with the invention, the surface of the tube wall is treated with a fusion inhibiting coating. Boron nitride has been found satisfactory in this regard and has successfully prevented the array of lengths from fusing to the inner surface of the outer glass tube. Preferably, the glass for the array of primary lengths has a slightly greater coefficient of thermal expansion than the outer tube glass. This choice of glasses provides a degree of compression during secondary heating that promotes fusion among the lengths because the air entrapped within the microchannels undergoes thermal expansion. It also enables the unfused outer tube to shrink away from the inner lengths while cooling. In this connection, it should be noted that fusion between the lengths and the tube causes the delicate lengths to crack as a consequence of the stresses established through cooling contraction.

In this secondary heating process, the entire assembly is suspended vertically once more in a furnace in order to combine the group of individual lengths into a fused array of microchannels. After cooling, the secondary product is cut transversely to produce a thin disc. An unfused glass ring that was cut from the outer tube is removed from the periphery of the disc. The microchannel structure then is placed in a vacuum in order to drive air out of the individual channels before it is immersed in an optical blocking or mounting wax. The wax fills the evacuated microchannels to prevent grinding and polishing debris from obstructing the channels and degrading the quality of the device. After grinding, the wax is heated and removed from the channels in order to produce a finished microchannel structure.

For a better understanding of the present invention together with other and further objects thereof, reference is had to the following description taken in connection with the accompanying drawings, the scope of the invention being pointed out in the appended claims.

BRIEF DESCRIPTION OF THE DRAWING FIG. 1 shows a typical apparatus for practicing the inventron;

FIG. 2 shows a hanger arrangement for individual tubes used in the embodiment of the invention;

FIG. 3 shows a typical apparatus for controlling the dimensions of the drawn product;

FIG. 4 shows a characteristic hexagonal length produced during a primary draw;

FIG. 5 is a representative embodiment of a typical finished product;

FIG. 6 is a representative embodiment of a typical sliced disc resulting from a secondary process; and

FIG. 7 is a schematic diagram of a typical furnace for carrying out the secondary process.

DESCRIPTION OF THE PREFERRED EMBODIMENTS FIG. I shows a typical apparatus for producing microchannel structures in accordance with the principles of the invention. The embodiment in FIG. I, moreover, illustrates a primary draw in which a large hexagonal bundle of cylindrical glass tubes are being drawn to a much smaller cross section in which a ratio of size reduction of 50 to l is typical. After the primary draw is finished, the primary lengths are sealed on both ends and grouped together for a second process that provides the final product. It has been found in this regard that Coming 8161 glass tubes of 0. I00 inch outside diameter are readily adapted to this process. Thus, as shown in FIG. 1, a modification of Atwood s machine (in which a weight 11 is connected through a cable 12 to a substantially airtight support 13 for a glass tube bundle 14) is used. The bundle 14 may contain 1,000 or more individual tubes. Preferably, the bundle of glass tubes has a hexagonal cross section. although other shapes also are suitable.

The cable 12 is passed over two sheaves 15 and 16. The bundle 14, moreover, is encased in a flexible, thermally insulating shroud 17 that depends from a vertically movable supporting member 20. The supporting member 20 is attached to an end of the cable 12 for vertical position control. The supporting member 20 also is connected through a conduit 21 to a vacuum pump (not shown) in order to establish a vacuum environment for the bundle 14.

The shroud 17 may comprise six flexible asbestos cloth members each parallel to and in physical contact with a respective one of the flat sides of the hexagonal bundle 14. This arrangement provides a sufficiently airtight enclosure for the bundle 14 during the primary draw.

A variable speed motor 22 and cable driving wheels 23 adjust the vertical position of the tube bundle 14. The motor speed is regulated as a function of the diameter of the bundle 14, the viscosity of the glass, and speed of the process to maintain an output volume that is equal to the volume of the bundle input to a furnace 24. v

As shown, the furnace 24 produces a vertical temperature gradient that increases with the height of the furnace. For example, a temperature of 1,175 F. at furnace top 26 has been found satisfactory. In this manner, convective air currents are eliminated within the furnace 24, inasmuch as the higher temperature at the furnace top 26 substantially prevents the development of vertical air motion.

The lower portion of the support 13 is nested within the upper portion of the furnace 24 to insure that the tube bundle 14 first reduces in size within the furnace in a bundle transitional portion 18. Should the bundle begin size reduction in the support 13, rather than in the furnace 24 as shown, the vacuum within the support will dissipate and produce undesirably collapsed channels under the influence of external atmospheric pressure. The conduit 21 that supports the tube bundle 14 passes through an airtight gland (not shown) in the top of the support 13. As shown schematically in FIG. 1, the furnace temperature gradient is controlled automatically through signals from thermocouples within the furnace 24 that are sent through conductor 27 to a furnace temperature gradient control circuit 30 that responds to these signals through the application of power to a cable 31 appropriate to the individual heating elements within the furnace.

A typical furnace for practicing the invention may have an interior height of 44 inches and an internal diameter of 18 inches. Twelve 1,000-watt heating elements arranged in a hexagon also are used in the furnace 24. This furnace, moreover, establishes a temperature gradient that illustratively may vary from 625 F. at the lower end ofthe furnace to about 1,1 75 F. at the furnace top 26. In order to distribute heat more uniformly within the lower portion of the furnace 24, a metal heat-modifying cylinder 28 is provided. The cylinder 28 circumscribes the flowing portion of the bundle 14 and extends through approximately the lower third of the furnace 24.

Under the influence of the furnace temperature and a drawing mechanism 32, the bundle 14 decreases in diameter and flows downwardly. An illustrative drawing mechanism 32 is shown below the furnace 24. It comprises a motor 33 that is connected to a chain drive drawing apparatus 34. The drawing apparatus 34 is equipped with high-temperature rubber grips 35 that pass over upper and lower pairs of sheaves 36 and 37 in order to enter opposing registration with each other and with a pulled" portion of the tube bundle 14. These pairs of grips draw the flowing portion of the bundle 14 vertically downward in lengths that are equal to a desired predetermined height of, for example, 15 inches.

Also coupled to the motor 33 are a pair of cutting edges 40. The cutting edges 40 are synchronized with the operation of the grips 35 to enable the cutting edge to slice off pulled segments of the bundle 14 at the point of engagement with the grips 35. Synchronizing the cutting edges 40 with the movement of the grips 35 reduces the wasted or damaged portion of each pulled length that is inherent in gripping and drawing the hot glass. After cutting, the primary draw lengths are received in a container 41 and are stored for subsequent processing.

In practicing the invention, the temperature gradient in the furnace 24 is maintained at a level in which the tube bundle 14 flows under the influence of the drawing mechanism 32, but has not melted. In this connection, the aforementioned temperature of about 1, F. at the top 26 of the furnace 24 has been found satisfactory when Coming 8161 glass is drawn.

The rate at which the primary draw progresses may be controlled visually through a Pyrex glass window (not shown) in the furnace 24. To keep the bundles transition zone 18 within the furnace, a switch 38 is operated to energize the motor 22 and lower the bundle into the furnace through an appropriate distance.

A typical apparatus for controlling the operation of the drawing mechanism 32 is shown in FIG. 3. An electric lamp 44 radiates a beam of light that is parallel to two of the flats in a pulled portion of the hexagonal glass bundle 14. Light beams traverse slits 45 and 46 that are formed between a collimator 47 and the opposing flats of the bundle 14.

These light beams are registered on the photosensitive surface of a photomultiplier tube 50. The photomultiplier tube 50 generates an electrical signal in response to changes in intensi- I ties in the light beams that are related to changes in the width of the slits 45 and 46 or the transverse distance D across the flats in the bundle 14. This signal is sent through a conductor 51 to a motor control circuit 52 that regulates the speed of the motor 33 to apply the appropriate drawing force to the flowing portion of the bundle 14 as the distance D increases or decreases beyond a predetermined range of, for example, 0.030 inch.

Ordinarily, the bundle 14 is suspended from the support 13 in the manner illustrated in FIG. 2. Two glass tubes 53 and 54 are fused to metal hangers 55 and 56, respectively. To enable the coefficient of thermal expansion of the hangers 55 and 56 to match that of the glass tubes 53 and 54, the hangers usually are made of Carpenter glass sealing metal as described in the book Carpenter, published in 1963 by the Carpenter Steel Co. of Reading, Pa. The Coming glass 8161, moreover, that is used in the illustrative embodiment of the invention, has a coefficient of thermal expansion of 88.1Xl0' inches/inch/ C. Each of the hangers 55 and 56 is provided with an enlarged area that protrudes from respective bulbous glass portions 58 and 59 formed in the sealed ends of the tubes 53 and 54. The bulbous portions 58 and 59 are exceptionally useful when all of the tubes are packed together in a hexagonal array. In this situation, stresses developed in the sealed tube ends may cause breakage at the narrow solid glass portions 48 and 49. The sealed integrity of the individual tubes 53 and 54, however, is not destroyed inasmuch as the broken narrow portions 48 and 49 do not place the interior surfaces of the hollow portions of the tubes in free communication with the vacuum established in the environment of the support 13.

FIG. 5 shows a typical microchannel disc 64. The disc 64 is produced through a secondary process that comprises assembling a group of hexagonal lengths 62 (FIG. 4) into a large array and fusing the microchannels 63 closed at both ends in each of the lengths 62. Air is thus sealed within all of the microehannels and prevents these microchannels from 001- lapsing during further processing as described subsequently.

The array of primary draw lengths is placed within a cylindrical glass tube (not shown) that has a higher melting point than that which characterizes the glass that forms the length 62. In this connection, Coming 7052 glass having a coefficient of expansion of 45 l0'"=" inches/inch/ C. has been found satisfactory for this purpose. Inasmuch as the individual lengths 62, when placed within the cylindrical glass tube, do not fully conform to a circular surface, void spaces between the peripheral lengths 62 and the inner surface of the glass tube are filled with solid rods of Coming 8 l6l glass that are of 0.030 inch to 0.010 inch in diameter. in order to prevent the individual lengths 62 from fusing to the annular glass tube, the inner surface of the tube is treated with a fusion inhibiting compound. For example, a coating of boron nitride has been found adequate to prevent this undesirable fusion between the two structures and the subsequent cracking in the component lengths that ordinarily would have occurred as a consequence of the stresses established during cooling and contraction.

The secondary process is accomplished in a different furnace 66 (FIG. 7). An outer glass cylinder 67 is suspended vertically in the furnace 66 through a flared top portion 70 that extends across a portion of the top of a carbon block 75 that rests on a ledge in a topmost heating zone 72.

it will be recalled that both ends of each length 73 from the primary draw were sealed in order to trap air within each of the microchannels. The glass cylinder 67 has a skirt portion 74 that extends below the lower ends of the lengths 73 and protrudes from the lower end of the furnace 66. A vacuum is drawn (not shown) in the tube skirt 74 to evacuate the interstices between each of the primary draw lengths 73. On reaching a temperature of about 580 C. in the heating zone 72, the sealed uppermost ends of the lengths 73 blow out. This blowout exposes the microchannels to atmospheric pressure, and squeezes together the outer surfaces of the individual lengths 73 under the vacuum in the tube 67 in order to preserve the vacuumtight integrity of the interstices at the upper end of the cylinder 67.

Thus exposed to atmospheric pressure on one side and a vacuum on the other side, the boundaries between each adjacent length close up to form a unified mass without crushing the boundary microchannels and producing an undesirable chicken wire effect. The temperature in heating zones 74 and 75 after blowout (which prior to blowout had been lower than the temperature in the zone 72) is gradually increased until it reaches about 545 C. At the same time, the zone 72 temperature is reduced to about 520 C. These relative temperatures are held for about 30 minutes to enable the common outer surfaces of the entire array of the lengths 73 to close up and fuse together. After fusion is complete along the entire array, temperatures in the zones 72, 74 and 75 are reduced gradually to room temperature. This heating procedure is controlled in the foregoing manner to insure atmospheric gas pressure within the channels. If any channel in the blown-out upper portion of the tube reseals, the gas pressure within that channel will increase to several atmospheres under the influence of the furnace temperature, causing at least some damage to the structure due to a burst microchannel.

The assembly in the glass cylinder 67 is not necessarily drawn for a further reduction in diameter. The array of lengths usually are treated in the forgoing manner only to fuse together and form a microchannel structure.

After the secondary process is complete, wafers 80 (FIG. 6) are sliced from the array with a thickness only slightly greater than that which is desired in the finished product. An outer ring 81 that is cut from the tube of Coming 7052 glass is removed from the microstructure disc, having been treated previously with boron nitride to prevent fusion with the drawn microstructure 82. As shown in FIG. 6, the microstructure 82 includes not only microchannels 83, but also peripheral groups of solid glass rods 84 that were used to fill the void spaces between the irregular periphery of the array of primary lengths and the cylindrical surface of the outer ring 81.

Turning once more to FIG. 5, the disc 64 is placed in a v three parts cerasin and one part rosin has been found suitable. The wax-filled disc is removed from the vacuum environment for grinding and finishing. Preferably, the microstructure is ground on a felt paper pad. The pad contains a grinding compound of which, for example, aluminum oxide and cerium oxide have been found satisfactory. The grinding compound grit should be either much larger or much smaller than the diameter of the microchannels. This choice of grit reduces the possibility of channel obstruction caused by grinding cornpound particles of diameters that are about the same size as the channels from becoming lodged in the microstructure. Thus, for example, cerium oxide having a grit size of 0.3 micron in a nonsettling suspension is well suited for this use.

After grinding is completed, the ground disc is warmed and the wax in the microchannels 65 is removed, the wax having served the purpose of keeping grit and other debris out of the channels during the grinding operation as well as providing structural support for the frail microstructure during the grinding process.

The microchannels are cleaned of wax and debris, for example, with Cobehn solvent (an anhydrous ethyl alcohol and trichloromethane solution) which has been put through a Soxhlet extractor. The extractor, moreover, is connected to a centrifuge in which the microchannel discs are placed at the extremities of the centrifuge rotor. In this way, the microchannels are subjected to fresh solvent flowing into the rotor from the extractor. The solvent is applied in this manner to the discs under centrifugal force and thus provides uniformly clean microchannels.

After the wax is removed, the disc 64 is ready for use. In the case of 8161 glass, moreover, it is preferable to keep the disc in a nitrogen atmosphere in order to prevent the glass structure from weathering.

it should be noted that the individual tubes from which the microstructure is made may have any suitable cross section. For example, rectangular and hexagonal inner and outer surfaces are suitable for use in connection with the invention, although circular cross sections have been shown in connection with the detailed description of the invention. Choice of glass, temperatures, specific expansion coefficients and the like, also are a flexible matter, depending on the sort of glasses that are selected for use in the process described. As an alternative to the use of a fusion-inhibiting compound between the tube and the group of primary lengths, a choice of structural materials that provide a mutually nonwetting surface between the lengths and the enclosing tube also is suitable.

What is claimed is:

1. in a method for producing a microchannel structure that involves the steps of inserting fused glass lengths of microchannels in a hollow glass member, drawing a vacuum within said member to the exclusion of said microchannels, heating the array of said lengths to cause said lengths to fuse together, wherein the improvement comprises the further step of treating said hollow glass member with a fusion-inhibiting coating of boron nitride to establish a fusion-inhibiting barrier between said member and said microchannel lengths to prevent said microchannel lengths from fusing to said member. 

